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Mates and Design 5 (2016) 231-255, Content its available at SeioncoDiroct Materials and Design ELSEVIER journal homepage: www.elsevier.com/locate/matdes Microstructural evolution of transition zone of clad X70 with duplex stainless steel Oe Xinjie Di*”, Zhentang Zhong °, Caiyan Deng *”*, Dongpo Wang *”, Xiaojiang Guo‘ * Sol of Maer Sees an ngnoering Tn Uns, ain 30072, china * Ta ey abr fae amok, an 3072 China * nace Eee LaboaaryTanspataan Sfy of O& as Ppt Lng 06500, hina ‘rl hy Receive 13 September 2013 Rec neve erm 2 ny 2018 ‘cept 20 any 2016 ‘able one 2 Janty 2016 ‘The microstructural evolution ofthe transition zone of clad X70 wit duplex stainless steel 2209 by hot-wire ‘tungsten inert gas T1G) welding was examined with an optical microscope (OM), scanning lecron microscope (SEN), and transmission electron microscope (TEM). The relationship beeen the ciuton rate, he value of ring the salificaton mode, an the mirostrtural evolution within the transition zone wer investigated ‘sing a Schell diagram and Fe-Cr-Nipseudobinary diagram It was found thatthe ution rate range from ‘to 14 within the wanton zone, causing variation in the value ofr Nn for0:36t0 255 Thetrasiion cond Sar wnrcanonedtaphstertes manesns arts manent se evince ma Mioharoess| ‘meta adjacent tothe fusion line, whe a hardened region was observed inthe clad aye. '© 2016 Eleever Lid Al rights reserve, 1. Introduction Cladding of duplex stainless steels (DSSs) on low-carbon or low- alloy stels is often use in the oi, petrochemical, nuclear, and marine industries, owing to their perfect combination of high tensile strength, good toughness, adequate weldabilty and stress-corrosion cracking re- sistance [1-3]. However, the joining of cissimilar materials is generally ‘more challenging than that of similar materials because of the difer- ences in the physical, chemical, mechanical, and metallurgical proper- ties ofthe metal welded, which make the dissimilar joints complicated. ‘The transition zone is a heterogeneous zone in dissimilar metal ‘welds Previous investigations indicated that the chemical composi- tions, microstructures, and physical and mechanical properties all change sharply across the transition zone [4-12]. Therefor, it is essen- tial to study the microstructural evolution ofthe transition zone fora better understanding f service performance. Reddy etal. [13] deposit- ed austenitic stainless steel on a high-strength low allay steel to study the structure and properties correlations. They discovered that the bond interface was nearly lat and the clad layer exhibited a dendritic austenite structure. Tensile strength and notch-tensile strength of the ‘base metal were higher than those ofthe weld overlay interface. Eghlimi 7 Corespondingauthr at Schoo of Matec Science and Engaceing. Tan Univers No. 92 Wein Ro Tn 300072, Cin "ma adie denganyanoiueducn (Den). neo 10.1016}marées201601.087 {G4-17510 2016 lire. Al ght resend. tal [14] added super-duplex stainless stet on high-strength low-alloy steel to evaluate the microstructure and texture across the welded inter- face. They pointed out that the major factors affecting the texture were ‘uncirectiona soliifcation, competitive growth, and 'yorientation rela- tionship. Lippold etal. [15] carried out the weld overlay cladding of ‘AISI8630 with Ni-base Alloy 625 to research the evolution of microstruc- tures that could promote a susceptibility to hydrogen-asssted cracking \with a variation inthe dilution rate across the transition zone. They con veyed that hydrogen-assisted cracking was most often associated with the planar growth zone and the formation of martensite owing to the extreme gradients in compositions. Kejelin et a. [16] pointed out that ‘transition zone formation was basically dependent on the chemical com positon ofthe welded meal dilution ofthe base metal, and the cooling "The dilution rate 's defined in terms ofthe change ofthe filer-metal composition by ‘mixing with the base metal [19]. The dilution rate within the transition zone can be determined by Eq, (1) [20]: « 2 X Dieta Matrs nd Desigh 95 (2016) 231-296 here D represents the dilution, Cis the concentration of any element within the transition zone Cy represents the nominal concentration of any element in the filer metal, and Cys the nominal concentration of fr severa investigations [5-16] have been conducted on the transition zone, the microstructural composition within the transition zone and the influence of the heat input on the microstructure are not clear. In particular, research studies on microstructural evolution by means of the solidification mode and solid-state transformation resulting from vatiations in the dilution rate are still limited. In order to understand the mechanism of premature failure and prevent the pre- ‘mature failure, further studies are necessary to provide more docu- ‘ments on the microstructural evolution details within the transition zone. nthe present study, an attempt was made to evaluate the chang- sof the solidification mode and the microstructural evolution with vat- iations inthe dilution within the transition zone, 2. Experimental procedures In the present study, cladding of DSS2209 on pipeline steel X70 (420 mm > 100 mm x 25 mm) was performed by hot-wire tungsten inert gas (TIG) welding. The chemical compositions ofthe base metal and overlay metal are given in Table 1, Before cladding, the base metal surface was ground and washed with acetone to remove oxide scales and contaminants. The cladding process parameters are summarized in Table 2. After the cladding process, some transverse samples were sliced from the clad composite for subsequent analysis. Specimens for micro- structural observation were prepared by standard mounting, grinding, and polishing methods. Then the base metal was etched with 4% Nital ‘hile the clad layer was etched with a solution of CuCls (5 g) + HCL (100 mi) + alcohol (100 ml). The metallographic microstructure of the transition zone was characterized by an optical microscope (OM) and scanning electron microscope (SEM). Moreover, the chemical com- position profile within the transition zone was analyzed by a SEM ‘equipped with Energy Dispersive X-ray Spectroscopy (EDS). A PHILIPS (€M200 transmission electron microscope (TEM) was used for analyzing, the microstructures’ characteristics of the transition zane ina more de- tailed way. The thin fils from the transition zone for TEM were pro- duced by twinjt polishing with 3% perchloric acd and 97% ethanol at temperatures ranging from ~25 °C to ~29 °C “Microhardness measurements across the transition zone were car ried out on the PM-ARS9000 Viekers microhardness testing machine with 2200 g lad and a holding time of 10 The cladding was conducted under three different heat inputs of (0.74 4mm, 133 klimm, and 1.93 klimm, The thesis mainly investigal- ed the microstructural evolution ofthe transition zone under optimal welding parameters (1.33 Km). 3. Results and analysis 2.1. Morphologies ofthe transition zone Fig 1a shows the OM image ofthe transition zone, which demon- strates that the interface of the base metal and clad layer was nearly flat. Fig. Tb shows a micrograph of the transition zane obtained by ‘SEM. The transition zone ean be divided into twa regions (named the "A" and "B" regions) bythe fusion line. In Fg, 1b line I represents adi- lution rate of 9%, ine ithe fusion line, and lines 3 and 4represent the boundaries offerent growth modes. The width ofthe “A” region is ap- proximately 5-7 um. The “B" region is composed of the zones of planar ‘and cellular growth. The widths ofthe planar and cellular zanes are ap- proximately 6-9 and 9-15 um, respectively. Owing tothe higher ther- ‘mal conductivity ofthe X70 substrate compared with that of DSS2208, large amounts of heat transfer and a steep temperature gradient existed near the fusion ine causing a lower constitutional supercooling. Hence, the zone adjacent to the fusion line was planar. Nevertheless as solii- fication proceeded, the base metal became warm. resulting ina gentle temperature gradient, and the constitutional supercooling increased, leading tothe domination of cellular structure growth [14 In situations ‘where the base metal and overlay metal were both ferritc at tempera- tures near the melting point, the solidification ofthe weld metal could always grow epitaxially from the unmelted or partially melted base ‘metal that served asthe nuclei, Thus, the cellular grains grew directly from the planar grains without the formation of border which is called “Typell grain boundaries in the overlay, as shown in Fig. 1b. 3.2, Composition profile within te transition zone SSEM-EDS was conducted to characterize the composition gradients ‘within the transition zone. Fig. 2a and b shows the chemical compost- tion profile ofthe transition zone of a heat input of 1.33 kj/mm. The ‘mass fraction ofthe major alloy elements in points 1 to 13 with an inter- ‘al of approximately 25 um in Fig. 2a is shown in Table 3. The dilution Fate of point 1 is approximately 99% as evaluated by the Fe element ac- cording to Eg, (1) Point sin the fusion ine with a dilution rate of 90%, Points 6 and 13 are on the boundaries of planar and cellular with a dilu- tion rate of 46% and 14% respectively. Fig. 2b, which isan example of, SEM-EDS line scans across the transition zone, shows that a bond of steep composition gradient was found within the transition zone. In the transition zone, Fe and Cr content varied markedly, while that of [Niincreased slower. The main reasons for these gradients were the ilu- tion of clad metal withthe base metal and the fast cooling rate ofthe ‘molten pool. Generally, the transition zone compesition was dependent ‘on the individual compositions of the base metal and overlay metal as ‘well a the dilution rate [19]. The transition zone covered a dilution ‘ate ranging from approximately 99% to 14%, Inaddition the dilution rate was related to the welding parame- ters. Fig. 2cand d shows the composition profile of a heat input of (0.74 kJ/mm, and Fig. 2 and F shows the composition profile of a heat input of 1.93 kj/mm. Although there was also a bond of steep ‘composition gradient across the transition zone, the composition gradient of the heat input of 1.93 k/mm was gentler, while that of 0.74 kl/mm was steeper compared with that of the heat input of 1.33 Kjmm, ‘bie ‘Cena composton fase metal and oe meal (Wt) Tenens a nine = & Mo @ W fe x00 Cr TT a bss mss kote 2302S 2X Dletal Mati nd Dein 95 2016) 231-296 2 ‘ible? Welding roe parameters. rameters Sheldng Wielding slow ate —_Fllerraddamexer Wot wire curent ‘Hotwire volage ‘Heat input 7 074 Kime 2 ream (99.99%) 15 Lin 12mm oA soy 133 Kim 3 153 im The microstructures within the transition zone are dependent on the dilution andthe cooling rate. The width of the transition zone of the lower heat input was narrower than that of the higher heat input (Fig. 22, ce). The elements segregated more seriously under the lower heat input so that each microstructure region became narrower. including the martensite region, while te higher heat input was the opposite. However, the phase balance of ferrite and austenite of the clad metal was upset when the heat input was lower or higher. 33, Microstructural evolution within the transition zone Despite its narrow width, there willbe a complicated microstructur- al evolution within the transition zone owing tothe deep gradient of alloy elements [5,11]. Although the Schaeffler diagram (Fig. 3) was developed to predict the weld metal constitution of stainless steels, it can also be applied to cording (o Fig. depending on the amount of the chemical composition ofthe transition zone normally cut across the composition range of ferrite + martensite (dilution >97%), ‘martensite (978 » dilution »598), ferrite + martensite (59% > dilation 39%) and austenite + martensite + frste (39% > dilution >14%) on the Schaeffler diagram. ‘TheTEM observation ofthe transition zoneis shown in Fig 4. Several, ‘mixed microstructure regions were observed within the transition MeN “bs ee Fig 1. Morphol ofthe anton zone (a) OM image ofthe imtrtae and () SEM icepap ef the deren gens zone: alpha ferite (ct) + martensite (M), M, M+ delta ferrite (6), and M+ austenite (9) + &asillustrated in Fig 4. Thus, the TEM results are consistent with the prediction ofthe Schaeler diagram. In Fig, 4a and ¢ the microstructures are both composed of Mand ferite although they are 6 and a, respectively, owing to different dilutions. The latice parameter of the ferrite in Fig, 4ais a 0.2931 nm, while that of Fig 4c is a = b = c = 0.3659 am. More alloy elements forming ferrite dissolved in &, which caused the lattice distortion of As can be een in Fig. 4b, the lath martensite exhibited their special appear ance, unlike those in homogeneous materials that divided the original austenitic into lath regions and hhad the same orientation [23]. The Width of the typical dislocation martensite lath was 0.08 yim to (0.58 umn, Fig. 4d indicated that martensite lath nucleated between the sain of delta ferrite and austenite because ofthe higher free energy of the grain boundary. In addition, there were no precipitates existing in the transition zone under the selected welding parameters 34, Microhardness measurements Fig. 5 shows the variations of Vickers microhardness across the tran- sition zone. Apparently, a dramati fluctuation in the microhardness can be seen across the transition zane. A softened region with a microhard- ness value of 236 HVo2 Was obtained in the base metal adjacent to the fusion line, while a hardened region with a microhardness value of 40H. was observed inthe cla layer. In ation, the microhardness of the base metal (276 HVp2) was alittle higher than that ofthe clad layer (259 Va) 4 Discussion ‘The cladding that developed during the fusion welding technique of issimilar alloys will achieve a chemical composition intermediate be- tween the two alloys {13,19}. The chemical composition will, in turn, havea significant influence on the solidification mode and mictostruc- tural evolution within the transition zone as well as its mechanical properties [224]. In general, for stainless see, to simplify a multi-component system, int the Fe-Cr-Ni temary system, Creg and Nixg were introduced and the solidification mode can be divided into the following four types [25,26 The dilution rate varied sharply within the transition zone. On aver- age, the dilution rate inthe “A” region was inthe range of 99% to 908, and the dilution rate in the “B” region ranged from 90% to 14% The var- {ation ofthe eitution will affect the value of Crey/Nix- According to the Fo-Ci-Ni pseudobinary phase diagram (Fig. 6) and the Schaefer mm Dieta Materia rd Design 95 (2016) 231-236 (Chemical Composition counts oeese see es 4 Chemica Composition cus ‘Chemical Compan coms g.2 £05 compotion assis ranston zane dierent het inputs: a). (b 139 Rn) (€) 074 aman (1.93 8m ‘able The mas action of major aly ements of eres pits (Wt) 4 ane Go 18 5 289, re) 305 6 7026 1436 an 4 1860 15% So ° 730 1236 5a 0 Dos 1780 558 CrajatCr+%4Mot 1 S%6Si40.5*96Nb " 215i eat 0 @ERI209 x70 rey aan 2 657 a aa a 857 Fag 3. sever dara for rising mest even thin the tras se concentration and light element character. These elements can be calcu lated by the dilution that canbe obtained by the concentration ofthe Fe element within the transition zone [20] AS long asthe variation in dilt- tion ofthe transition zones known, together with the nominal concen: trations of alloy elements ofthe overlay metal and base metal, the C,N, Cu. Si, and Nb can be obtained by back-calculation. Of course, the hy: pothesis ofthis method is that C, N,Cu, Si and Nb will be mixed in the liquid stat tothe same level within the transition zone asthe Fe ele- ‘ment. The variation in dilution evaluated by the Fe element within the transition zone is determined by Ea. (1). Thus, the mass fraction of Jow concentration and light elements can be calculated by Eq, (4) [19], ‘nce the dilution within the transition zone is known, Co = Dim + (1D IC @ Therefore, Cay and Nig wil be obtained with the concentration of relevant elements. The dilution rate, the Cray/Nix Vale, the sliifica- fasion line (the clad layer side is positive, while the base metal is nega tive) within the transition zone are shown in Table 4 in deta Table 4 shows that martensite existed in all four regions. As previous, studies indicated [8.20.21 28], the formation of intermediate composi tions with high hardenabilty such as Cr and Ni (shown in Fig. 2b), {and the rapid cooling rate caused the formation of martensite. More: over, the lath martensite regions appeared “jumbled” in an original austenitic grain because the Mi, points varied with distance fromthe f- som line, a illustrated in Fig. 4b In addition, the martensite layer was greatly dependent on the local hardenabilty (as determined by local Composition) and loca cooling rate (20). According to Fig. 3, martensite can form only ata dilution above 14%, and single-phase martensite can form only ata dilution between 59% and 97% located approximately ‘34m from the fusion line inthe clad layer. (CtegNigg —* tion mode the microstructural evolution, and the distance fom the 5128 148 195262 40 10005128188 6 of) =a-Bliberhes anes tu Gmaiion aee 1400 I 460 is. : io] Tit = oan fl B 1200 mv 320 4 § ae ie § Vee {sso & 1000 it | : £ ot : im \ 8 ; soo : a ieoy : : A RH FAI ' t eos 00 F | 1 eo ino | yon | i | 1 x x c : 20 : x cf ~— = : : fusion line (um gS. Vrtion of Vier: Micardis aro the tration one Fis. 6 Relative postion of fur slifcation mes of duplex stanes sts in = x6 Dieta Materia rd Design 95 (2016) 231-236 Dusan in) Dion (8) Cra/Ng Seaton mode Micosmares 30 rr aM as 16 fA M 50 am F Mae 15 bas Mie 100 ais Mie 125, 2 yom 150 236 yet 5 2 VM ws 20 F TEM 3 Pe yews. Tor the single-phase martensite region, ‘elements increased sharply it covered a dilution ap- proximately from 90% to 75% causing a solidification mode ranging, from A to FA In regard to the A solidification mode, austenite was the primary solidification phase, and the solid-state transformation of aus- fenite to martensite would process after the completion of primary aus- {enite solidification. ln regard to single-phase martensite region from the FA solidification mode, after both the primary and eutectic ferrite completely transformed into austenite, all austenite transformed into martensite under the cooling rate exceeding the citical cooling rate. With the dilution decreasing, the value of Creq/Nieg increased and the solidification mode changed to the F mode. The M+ and y+ M+ regions were both F solidification mode in which the pri- ‘mary ferrite was the only phase. Then the solid-state transformation of austenite to martensite proceeded after some primary ferrite transformed into austenite. The transformation of austenite to martensite proceeded fully in the M + region, while that of the 7 5.Condlusions ‘This study addressed the microstructural evolution within the tran- sition zone of D552209 cladding on pipeline stel X70. The main conclu- sions areas follows: (1) The main growth mode ofthe transition zane was the epitaxial nucleation with planar growth adjacent tothe fusion line that shift to cellular growth, (2) The major alloy elements Fe, Cr, and Nihad a bond of steep com- position gradient within the transition zone. The dilution est: ‘mated by the Fe element within the transition zone ranged (4) A dramatic fuctuaton in the microhardness existed within the transition zone, which was consistent with the microstructural evolution. A softened region was obtained in the base metal ad- Jacent tothe fusion line while a hardened region was observed in the cla layer: References (0) ero, oar) loll, Mere M. Maras influence hemi cm ‘ion on he iting corrosion esac natn aN ih Ms lx tet Coos S45 (2S) 09-321, [2] NRC Bao Sains sel in corto: ee a esac spins cha Jeng nd opps Constr ste Re 4 (208) 119-1208 (5) 8 ener dans Cory A os Sales see renforcngbr reason for thir ‘gh png coeson ressance, Mar Cras 62 (2011) 111-119. 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